An Efficient, Robust New Scheme for Establishing Broadband Homonuclear Correlations in Biomolecular Solid State NMR.,ChemPhysChem

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An Efficient, Robust New Scheme for Establishing Broadband Homonuclear Correlations in Biomolecular Solid State NMR.
ChemPhysChem ( IF 2.3 ) Pub Date : 2020-01-16 , DOI: 10.1002/cphc.201901071
Sungsool Wi ₁ , Lucio Frydman _{1,

2}

Affiliation

An efficient mixing scheme is introduced for establishing two‐dimensional (2D) homonuclear correlations based on dipolar couplings. This mixing scheme achieves broadband dipolar recoupling using remarkably low powers even under ultrafast magic‐angle spinning (MAS) rates. This Adiabatic Linearly FREquency Swept reCOupling (AL FRESCO) method applies a series of weak frequency‐chirped pluses on the ¹H channel, for performing efficient ¹³C−¹³C magnetization transfers leading to cross peaks between sites separated over small or large chemical shift differences. The mixing scheme is nearly free from dipolar truncation effects, and thanks to the low RF powers it involves it can act over long mixing times (≥1.5 sec). Key considerations required for optimizing this chirped pulse mixing scheme are discussed, and the new kind of correlations that can emerge from this method are demonstrated using uniformly ¹³C‐labeled Barstar as test protein sample.

中文翻译：

在生物分子固态NMR中建立宽带同核相关性的高效，稳健的新方案。

为了建立基于偶极耦合的二维（2D）同核相关性，引入了一种有效的混合方案。即使在超快幻角旋转（MAS）速率下，这种混频方案也能以非常低的功率实现宽带偶极耦合。这种绝热线性频率扫频重耦合（AL FRESCO）方法在¹ H通道上应用了一系列弱频率chi脉冲，以执行有效的¹³ C− ¹³C磁化转移导致在因小或大化学位移差异而分开的位点之间出现交叉峰。混合方案几乎没有偶极截断效应，并且由于其低射频功率，它可以在较长的混合时间（≥1.5秒）内起作用。讨论了优化此chi脉冲混合方案所需的关键注意事项，并使用¹³ C标记的Barstar均匀地作为测试蛋白样品，证明了该方法可能产生的新型相关性。

更新日期：2020-01-16

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